Synthetic Route of 14482-51-0, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.14482-51-0, name is 2-Bromo-3,5-dichloropyridine, molecular formula is C5H2BrCl2N, molecular weight is 226.89, as common compound, the synthetic route is as follows.
Raw material selection: 17.5 g of 2-bromo-3,5-dichloropyridine, 34.54 g of cuprous cyanide (CuCN), 12.6 g of 2-methylimidazole,The reaction organic solvent dimethylacetamide (DMSO) 105 ml; purified organic solvent n-heptane 100 ml.In the process of extracting and washing the organic solvent (or ethyl acetate or toluene or cyclohexane or petroleum ether) after the completion of the reaction, the amount of the organic solvent and the amount of water are conventional and not limited; the following specific process is toluene Extraction is an example.Reaction step: 17.5 g of 2-bromo-3,5-dichloropyridine prepared above, 34.54 g of cuprous cyanide (CuCN), 12.6 g of 2-methylimidazole were added to a dry 250 ml reaction flask, and an organic solvent was added. 105 ml of dimethylacetamide was heated to 105-110 C under the protection of nitrogen, and the reaction was completely cooled to room temperature.Add 150 ml of toluene in an organic solvent, stir for about 10 minutes, add 100 ml of water, filter the solid, separate the organic phase from the filtrate, and wash the residue twice with toluene (50 ml/time).The washing liquid continues to extract the aqueous phase, and the liquid phase is separated, and the organic phase is combined, washed once with 100 ml of water, and evaporated to dryness under reduced pressure at 60 C in a water bath.Producing a crude solid of 3,5-dichloro-2-cyanopyridine;The crude solid of 3,5-dichloro-2-cyanopyridine obtained is recrystallized from purified organic solvent n-heptane: 100 ml of n-heptane is added and heated to 90 C to dissolve, and then slowly cooled to about 10 C to precipitate a solid, and the product is obtained by filtration. ,Drying at 40-60 C under vacuum gave 9.1 g of 3,5-dichloro-2-cyanopyridine, the yield was 68.2%, the product purity was 99.2%, and the total reaction yield was 64.4%.
The chemical industry reduces the impact on the environment during synthesis 14482-51-0, I believe this compound will play a more active role in future production and life.
Reference:
Patent; Hangzhou East China Pharmaceutical Group Zhejiang Huayi Pharmaceutical Co., Ltd.; Weifang Haixin Pharmaceutical Co., Ltd.; Lou Qingming; Wu Lei; Lou Lei; (8 pag.)CN109020882; (2018); A;,
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